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At least 37 records · Page 2Linked to original sources
USGS1988

High-performance liquid-chromatographic separation of subcomponents of antimycin-A

Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, A 1a , A 1b , A 2a , A 2b , A 3a , A 3b , A 4a , and A 4b . Although a base-line resolution of the known four major antimycins A 1 , A 2 , A 3 , and A 4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

Journal of Chromatography↗
USGS1993

Determination of size and element composition distributions of complex colloids by sedimentation field-flow fractionation—inductively coupled plasma mass spectrometry

Sedimentation field-flow fractionation (SdFFF) and inductively coupled plasma mass spectrometry (ICP-MS) have been directly combined and the resulting SdFFF-ICP-MS instrument can be used to produce element based size distributions of colloidal samples. Using appropriate tracer elements the size distributions of specific components can be picked out from a complex mixture. Changes in chemical composition of mixtures as a function of particle size can be readily monitored by plotting appropriate element atomic ratio distributions. These applications have been illustrated using data obtained with samples of the clay minerals kaolinite and illite and a natural suspended particulate matter from the Darling River (Australia).

Journal of Chromatography A↗
USGS1993

Application of mixed-mode, solid-phase extraction in environmental and clinical chemistry. Combining hydrogen-bonding, cation-exchange and Van der Waals interactions

Silica- and styrene-divinylbenzene-based mixed-mode resins that contain C8, C18 and sulphonated cation-exchange groups were compared for their efficiency in isolation of neutral triazine compounds from water and of the basic drug, benzoylecgonine, from urine. The triazine compounds were isolated by a combination of Van der Waals and hydrogen-bonding interactions, and benzoylecgonine was isolated by Van der Waals interactions and cation exchange. All analytes were eluted with a polar organic solvent contaning 2% ammonium hydroxide. Larger recoveries (95%) were achieved on copolymerized mixed-mode resins where C18 and sulfonic acid are in closer proximity than on 'blended' mixed-mode resins (60-70% recovery).

Journal of Chromatography A↗
USGS2015

Determination of 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene and related compounds in marine pore water by automated thermal desorption-gas chromatography/mass spectrometry using disposable optical fiber

A method is described for determination of ten DDT-related compounds in marine pore water based on equilibrium solid-phase microextraction (SPME) using commercial polydimethylsiloxane-coated optical fiber with analysis by automated thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS). Thermally cleaned fiber was directly exposed to sediments and allowed to reach equilibrium under static conditions at the in situ field temperature. Following removal, fibers were rinsed, dried and cut into appropriate lengths for storage in leak-tight containers at -20°C. Analysis by TD-GC/MS under full scan (FS) and selected ion monitoring (SIM) modes was then performed. Pore-water method detection limits in FS and SIM modes were estimated at 0.05-2.4ng/L and 0.7-16pg/L, respectively. Precision of the method, including contributions from fiber handling, was less than 10%. Analysis of independently prepared solutions containing eight DDT compounds yielded concentrations that were within 6.9±5.5% and 0.1±14% of the actual concentrations in FS and SIM modes, respectively. The use of optical fiber with automated analysis allows for studies at high temporal and/or spatial resolution as well as for monitoring programs over large spatial and/or long temporal scales with adequate sample replication. This greatly enhances the flexibility of the technique and improves the ability to meet quality control objectives at significantly lower cost.

Journal of Chromatography A↗
USGS2016

Determination of polydimethylsiloxane–water partition coefficients for ten 1-chloro-4-[2,2,2-trichloro-1-(4-chlorophenyl)ethyl]benzene-related compounds and twelve polychlorinated biphenyls using gas chromatography/mass spectrometry

Polymer-water partition coefficients (Kpw) of ten DDT-related compounds were determined in pure water at 25 °C using commercial polydimethylsiloxane-coated optical fiber. Analyte concentrations were measured by thermal desorption-gas chromatography/full scan mass spectrometry (TD–GC/MSFS; fibers) and liquid injection-gas chromatography/selected ion monitoring mass spectrometry (LI–GC/MSSIM; water). Equilibrium was approached from two directions (fiber uptake and depletion) as a means of assessing data concordance. Measured compound-specific log Kpw values ranged from 4.8 to 6.1 with an average difference in log Kpw between the two approaches of 0.05 log units (∼12% of Kpw). Comparison of the experimentally-determined log Kpw values with previously published data confirmed the consistency of the results and the reliability of the method. A second experiment was conducted with the same ten DDT-related compounds and twelve selected PCB (polychlorinated biphenyl) congeners under conditions characteristic of a coastal marine field site (viz., seawater, 11 °C) that is currently under investigation for DDT and PCB contamination. Equilibration at lower temperature and higher ionic strength resulted in an increase in log Kpw for the DDT-related compounds of 0.28–0.49 log units (61–101% of Kpw), depending on the analyte. The increase in Kpw would have the effect of reducing by approximately half the calculated freely dissolved pore-water concentrations (Cfree). This demonstrates the importance of determining partition coefficients under conditions as they exist in the field.

Journal of Chromatography A↗
USGS2000

Considerations involved with the use of semipermeable membrane devices for monitoring environmental contaminants

Semipermeable membrane devices (SPMDs) are used with increasing frequency, and throughout the world as samplers of organic contaminants. The devices can be used to detect a variety of lipophilic chemicals in water, sediment/soil, and air. SPMDs are designed to sample nonpolar, hydrophobic chemicals. The maximum concentration factor achievable for a particular chemical is proportional to its octanol–water partition coefficient. Techniques used for cleanup of SPMD extracts for targeted analytes and for general screening by full-scan mass spectrometry do not differ greatly from techniques used for extracts of other matrices. However, SPMD extracts contain potential interferences that are specific to the membrane–lipid matrix. Procedures have been developed or modified to alleviate these potential interferences. The SPMD approach has been demonstrated to be applicable to sequestering and analyzing a wide array of environmental contaminants including organochlorine pesticides, polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polychlorinated dioxins and dibenzofurans, selected organophosphate pesticides and pyrethroid insecticides, and other nonpolar organic chemicals. We present herein an overview of effective procedural steps for analyzing exposed SPMDs for trace to ultra-trace levels of contaminants sequestered from environmental matrices.

Journal of Chromatography A↗
USGS1982

High-performance liquid chromatographic resolution and quantification of a dilacton antibiotic mixture (antimycin A)

High-performance liquid chromatographic (HPLC) conditions are presented for the separation and quantitative determination of a homologous antibiotic complex (antimycin A). Combined HPLC and chemical ionization mass spectrometry proved to be exceptionally useful for the structural identification of chromatographic components. Using electrochemical, fluorescence, and ultraviolet detectors, the minimum detectable amounts of the antibiotics were found to be in the ranges 0.10–1.12, 0.31–1.69, and 4.10–28.2 ng, respectively. Advantages of the preparation of Dns derivatives for use in fluorescence detection are discussed. Application of the HPLC technique to the analysis of the antibiotic mixture in organic tissues is demonstrated.

Journal of Chromatography↗
USGS1985

Retention behavior of long chain quaternary ammonium homologues and related nitroso-alkymethylamines

Several chromatographic methods have been utilized to study the retentionbehavior of a homologous series of n -alkylbenzyldimethylammonium chlorides (ABDAC) and the corresponding nitroso- n -alkylmethylamines (NAMA). Linear correlation of the logarithmic capacity factor ( k ') with the number of carbons in the alkyl chain provides useful information on both gas chromatographic (GC) and high-performance liquid chromatographich (HPLC) retention parameters of unknown components. Under all conditions empolyed, GC methodology has proved effective in achieving complete resolution of the homologous mixture of NMA despite its obvious inadequacy in the separation of E-Z configurational isomers. Conversely, normal-phase HPLC on silica demonstrates that the selectivity (a) value for an E-Z pair is much higher than that for an adjacent homologous pair. In the reversed-phase HPLC study, three different silica-based column systems were examined under various mobile phase conditions. The extent of variation in k ' was found to be a function of the organic modifier, counter-ion concentration, eluent pH, nature of counter-ion, and the polarity and type of stationary phase. The k '—[NaClO 4 ] profiles showed similar trends between the ABDAC and the NAMA series, supporting the dipolar electronic structures of the latter compounds. Mobile phase and stationary phase effects on component separation are described. The methodology presented establishes the utility of HPLC separation techniques as versatile analytical tools for practical application.

Journal of Chromatography↗
USGS1998

Loading capacity and chromatographic behavior of a porous graphitic carbon column for polychlorinated biphenyls

A porous graphitic carbon column (Hypercarb) was used for the fractionation of polychlorinated biphenyls (PCBs) into classes of 2-4 ortho chlorines, 1 ortho chlorine and 0 ortho chlorine congeners. A method was developed that combined the fractionation of PCBs, polychlorinated dibenzo- p -dioxins and dibenzofurans in a variety of biotic environmental samples. Many of these samples have high concentrations of PCBs which cause fractionation problems as adsorption sites on the graphitic surface are occupied. The loading capacity of the column for PCBs was determined by injecting up to 1 mg of total PCBs and monitoring changes in chromatographic behavior of tetra-/di- ortho , mono- ortho and non- ortho substituted PCBs. Effective loading capacities were 1 mg for tetra-/di- ortho PCBs, but only 3–5 μg for non- ortho PCBs and about 2 μg for mono- ortho PCBs. Loading capacity of the PGC column for environmental fish and avian egg samples was determined to depend on the mono- ortho and non- ortho PCB levels found in these samples.

Journal of Chromatography A↗
USGS1999

Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., <14%), and sensitivity (method quantitation limit, <24 ng/g) for each analyte indicate the usefulness of this method for studies characterizing the depletion of benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

Journal of Chromatography A↗
USGS1989

Reversed-phase high-performance liquid chromatography of unsubstituted aminobenzoic acids

High-performance liquid chromatographic (HPLC) characteristics of three position isomers of aminobenzoic acids (potential metabolites of important anesthetic drugs), were delineated with respect to their interactions with various mobile phases and stationary phases. HPLC with five hydrocarbonaceous phase, I?-cyclodextrin silica (CDS), macrophase MP-1 polymer (MP), macroporous polystyrene/divinylbenzene (MPD), octadecylsilica (ODS), and propylphenylsilica (PPS), yielded results explicable in terms of substituent effects derived from the bifunctional amino- and carboxy groups. For cases where mobile phases contained sulfonates or quaternary ammonium salts both having longer chain alkyls, retention of analytes on all but CDS appeared to proceed predominantly via an ion-pairing mechanism. The extent of the corresponding counter-ion effects decreased in the order: MPD > ODS > PPS > MP, while the analyte retention order paralleled thier pH 2 values. On the other hand, an inverse relationship between the magnitude of capacity factors (k') and pK 1 values of the title compounds was observed in experiments that produced retention data incompatible with ion-pair interaction rationales. The unique HPLC results obtained with the CDS phase are compared with those obtained with other phases.

Journal of Liquid Chromatography↗
USGS2005

Kovats and lee retention indices determined by gas chromatography/mass spectrometry for organic compounds of environmental interest

Retention indices of standard organic compounds of environmental interest were determined by gas chromatography/mass spectrometry, using a DB‐5 fused‐silica capillary column. Retention indices are useful references for tentative compound identification by gas chromatography, or confirmation by gas chromatography/mass spectrometry. They provide elution order for isomers that might be indistinguishable based on mass spectra. Modified Kovats and Lee retention indices are given for polycyclic aromatic hydrocarbons; sulfur heterocycles; nitrogen heterocycles; aromatic amines; oxygen heterocycles; phenols; alcohols; ketones; alkanes; nitriles; and methylesters of fatty, dicarboxylic, and aromatic acids for comparison and reference. Retention index values for heterocycles by gas chromatography/mass spectrometry are comparable with gas chromatography values previously reported.

Journal of Separation Science↗
USGS2020

Gas-liquid chromatographic and gas-liquid chromatographic-mass spectrometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

Journal of the Association of Official Analytical ↗
USGS2020

GLC determination of quinaldine residue in fish

A procedure for the determination of quinaldine residue in various fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether, the extracts are concentrated by partitioning through 0.1N sulfuric acid, and the residues are measured by alkali flame ionization gas chromatography. Muscle tissues containing from 0.01 to 10.0 ppm quinaldine were successfully analyzed with recoveries from 75 to 100%.

Journal of the Association of Official Analytical ↗
USGS1975

Radiochemical determination of very low concentrations of nickel in rocks and minerals

A radiochemical procedure has been developed for the determination of very low concentrations of nickel in rocks and minerals. Sensitivity is 0.01 μ g Ni. Accuracy and precision is estimated to be ±5 percent to levels as low as 0.1 μ g Ni a marked improvement over other analytical techniques. Samples are irradiated, combined with nickel carrier, and treated by a series of chemical procedures: (1) collection of nickel in a lead bead using a fire-assay technique, (2) refusion of the lead bead and precipitation of basic element hydroxides, (3) anion-exchange chromatography, and (4) precipitation of nickel dimethylglyoxime. The nickel precipitate is weighed to determine chemical yield and counted for β activity of Ni 65 along with a precipitate from irradiated nickel standard solution.

Journal of Research of the U.S. Geological Survey↗